CN102898806A - Antistatic polycarbonate/polyester alloy material and preparation method thereof - Google Patents
Antistatic polycarbonate/polyester alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of antistatic polymers, in particular to a polycarbonate/ polyester alloy material and a preparation method thereof. The antistatic polycarbonate/ polyester alloy material comprises the following components in percentage by weight: 5 to 25 percent of conductive carbon black, 50 to 70 percent of polycarbonate, 10 to 30 percent of polyester, 0. 01 to 0.05 percent of ester exchange catalyst, 1 to 4 percent of compatilizer, 0.1 to 0.5 percent of antioxidant and 0.2 to 1 percent of lubricant; and the preparation method comprises the following steps of: mixing the compatilizer, the ester exchange catalyst, the antioxidant, the heat stabilizer and the lubricant in a high-speed mixing machine; putting the mixture with the polycarbonate and the polyester into an internal mixer until the mixture is molten; and putting the conductive carbon black into the internal mixer, feeding the melt into a twin screw extruder for melt extrusion and prilling. By the method, the prepared alloy material has good performance, good solvent performance and low melt viscosity, stress crack is avoided, and the raw material cost is reduced.
Description
Technical field
The present invention relates to the anti-electrostatic polymer field, relate in particular to a kind of polycarbonate/polyester alloy material and preparation method thereof.
Background technology
Polycarbonate is very widely thermoplastic engineering plastic of a kind of application, has rigidity large, the advantages such as Young's modulus is high, Heat stability is good, and size is stable make it obtain wide application at electronic enterprises such as machinery, tool outer casing, body, computer and televisors.Polycarbonate is electrical insulator, easily produces static and causes electronic apparatus to damage, and for the loss that prevents from causing because of static, it can be combined with electro-conductive material.Disclose in more existing data and partly adopted carbon fiber, graphitized carbon black, carbon nanotube etc. to join preparation anti-static polycarbonate material in the polycarbonate material as electro-conductive material.In view of source, price and the technology maturation of electro-conductive material, at present, it is main that the conductive filler material that dominates in the world market is still graphitized carbon black.
Although it is large that polycarbonate has rigidity, Young's modulus is high, Heat stability is good, the advantages such as size is stable, but its solvent resistance is relatively poor, melt viscosity is high, stress cracking easily appears, particularly in preparation anti-static polycarbonate process, need a large amount of electro-conductive materials to be added in the matrix resin, cause anti-static polycarbonate moulding difficulty, and the melt viscosity of polyester is relatively low, prepared film or sheet material folding, number of bends can reach 100,000 times, the price of polyester is also low than polycarbonate, therefore polycarbonate and polyester blend are developed excellent heat stability, solvent resistance is strong, anti-static polycarbonate/the polyester alloy of stress crack resistant has actual using value, but the crystal property of polycarbonate and polyester exists greatest differences, compatibility performance is not good enough, has affected the practical application of polycarbonate and polyester blend system.
Summary of the invention
Technical problem to be solved by this invention provides a kind of anti-static polycarbonate/polyester alloy material and preparation method thereof, and the polycarbonate solvent resistance is relatively poor in the prior art, melt viscosity is high to solve, the stress cracking shortcoming such as higher relative to price easily occur.
The present invention is achieved in that a kind of anti-static polycarbonate/polyester alloy material, and this material comprises following component graphitized carbon black 5 ~ 25%, polycarbonate 50 ~ 70%, polyester 10 ~ 30%, transesterification catalyst 0.01 ~ 0.05%, compatilizer 1 ~ 4%, oxidation inhibitor 0.1 ~ 0.5%, lubricant 0.2 ~ 1% by weight percentage;
Described compatilizer is the dihydroxyphenyl propane solid epoxy; Described polycarbonate is bisphenol-a polycarbonate.
Also comprise by weight percentage 0 ~ 5% thermo-stabilizer in this material.
Described polyester is ethylene glycol, hexylene glycol, propylene glycol, butyleneglycol, 1, one or more arbitrary proportion combinations in 4-cyclohexanedimethanol, neopentyl glycol and the terephthalyl alcohol and one or more arbitrary proportion combinations in terephthalic acid, m-phthalic acid, cyclohexane cyclohexanedimethanodibasic, pentanedioic acid, hexanodioic acid and the suberic acid, the copolyesters that carries out polymerization.
The melting index of described polycarbonate is 3 ~ 15 g/10min (300 ℃/1.2kg, ISO1133).
The DBP absorption value of described graphitized carbon black is that 300 ~ 600ml/100g (ASTM D 2414), resistance are less than 150 Ω cm(Philips-Method), tap density is greater than 120g/l (ASTM D 1513).
Described dihydroxyphenyl propane solid epoxy, its epoxy equivalent (weight) are 800 ~ 3500g/eq (GB/T 4612-2008).
Described transesterification catalyst is a kind of or its combination in Dibutyltin oxide, Mono-n-butyltin, Mono-n-butyltin muriate, monobutyl three isocaprylic acid tin, dibutyl tin acetate, Glacial acetic acid cerium, acetyl ethyl ketone cerium, Glacial acetic acid lanthanum and the acetyl ethyl ketone lanthanum.
Described oxidation inhibitor is tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester, two (2, the 4-di-tert-butyl-phenyl) tetramethylolmethane diphosphorous acid fat, four [3-(3,5-di-t-butyl-4-hydroxyphenyl) propionic acid] quaternary amyl alcohol ester, β-(4-hydroxy phenyl-3, the 5-di-t-butyl) the positive octadecanol ester of propionic acid, 2, the 6-di-tert-butyl-4-methy phenol, 2,2 ' methylene radical-two (4-methyl-6-tert-butylphenol), 4,4 '-thiobis (the 6-tertiary butyl-3-methylphenol) or 4, one or more arbitrary proportion combinations in 4 '-thiobis (6-tertiary butyl meta-cresol).
A kind of as claimed in claim 1 anti-static polycarbonate/polyester alloy material preparation method may further comprise the steps:
1) with 1 ~ 4% compatilizer, 0.01 ~ 0.05% transesterification catalyst, 0.1 ~ 0.5% oxidation inhibitor, 0 ~ 5% thermo-stabilizer and 0.2 ~ 1% lubricant high-speed mixer and mixing 10 ~ 20 minutes;
2) mixture, 50 ~ 70% polycarbonate and 10 ~ 30% polyester with step 1 gained drop in the Banbury mixer, until melting;
3) 5 ~ 25% graphitized carbon blacks are dropped in the Banbury mixer, the kneading time is 5 ~ 8 minutes, and temperature is 270 ~ 290 ℃;
4) melt that step 3 is obtained is sent in the twin screw extruder, and the rotating speed of forcing machine is 150 ~ 300 rev/mins, melt extrudes granulation under 260 ~ 280 ℃ of temperature.
Also comprise before the described step 1 polycarbonate, polyester and graphitized carbon black 100 ~ 110 ℃ of steps of lower dry 12 ~ 24 hours.
Anti-static polycarbonate of the present invention/polyester alloy material and preparation method thereof utilizes and contains the structure of bisphenol A unit the same with polycarbonate in the solid epoxy, and its hydroxyl and epoxy active function groups can with polycarbonate and polyester in carbonate group, ester group, the terminal hydroxy group characteristics of reacting, take Resins, epoxy as compatilizer, in conjunction with the Exchange Ester Process of polycarbonate and polyester, prepare high performance anti-static polycarbonate/polyester alloy material; Compare with existing material and to have advantages of that solvent nature is good, melt viscosity is low, be not prone to stress cracking, and reduced raw materials cost; The prepared alloy material of the present invention can be used for plastic part, film and sheet material, is widely used in machinery and the field of electronics higher to the size stability requirement.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's statement, these equivalent form of values fall within the application's appended claims limited range equally.
The invention provides a kind of anti-static polycarbonate/polyester alloy material, this material comprises following component graphitized carbon black 5 ~ 25%, polycarbonate 50 ~ 70%, polyester 10 ~ 30%, transesterification catalyst 0.01 ~ 0.05%, compatilizer 1 ~ 4%, oxidation inhibitor 0.1 ~ 0.5%, lubricant 0.2 ~ 1% by weight percentage, and described compatilizer is the dihydroxyphenyl propane solid epoxy; Described polycarbonate is bisphenol-a polycarbonate; And add 0 ~ 5% thermo-stabilizer according to actual requirement and situation selectivity.
Wherein, described thermo-stabilizer is one or more arbitrary proportion combinations of trimethyl phosphite 99, triethyl phosphate, triphenylphosphate and triphenyl phosphite.
Described polyester is ethylene glycol, hexylene glycol, propylene glycol, butyleneglycol, 1, one or more arbitrary proportion combinations in 4-cyclohexanedimethanol, neopentyl glycol and the terephthalyl alcohol and one or more arbitrary proportion combinations in terephthalic acid, m-phthalic acid, cyclohexane cyclohexanedimethanodibasic, pentanedioic acid, hexanodioic acid and the suberic acid, carry out the copolyesters of polymerization, its limiting viscosity is 0.75 ~ 1.2dL/g(GB/T 14190-2008).
The melting index of described polycarbonate is 3 ~ 15 g/10min (300 ℃/1.2kg, ISO1133).
The DBP absorption value of described graphitized carbon black is that 300 ~ 600ml/100g (ASTM D 2414), resistance are less than 150 Ω cm(Philips-Method), tap density is greater than 120g/l (ASTM D 1513).
The epoxy equivalent (weight) of described dihydroxyphenyl propane solid epoxy is 800 ~ 3500g/eq (GB/T 4612-2008).
Described transesterification catalyst is a kind of or its combination in Dibutyltin oxide, Mono-n-butyltin, Mono-n-butyltin muriate, monobutyl three isocaprylic acid tin and dibutyl tin acetate, Glacial acetic acid cerium, acetyl ethyl ketone cerium, Glacial acetic acid lanthanum and the acetyl ethyl ketone lanthanum.
Described oxidation inhibitor is tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester, two (2, the 4-di-tert-butyl-phenyl) tetramethylolmethane diphosphorous acid fat, four [3-(3,5-di-t-butyl-4-hydroxyphenyl) propionic acid] quaternary amyl alcohol ester, β-(4-hydroxy phenyl-3, the 5-di-t-butyl) the positive octadecanol ester of propionic acid, 2, the 6-di-tert-butyl-4-methy phenol, 2,2 ' methylene radical-two (4-methyl-6-tert-butylphenol), 4,4 '-thiobis (the 6-tertiary butyl-3-methylphenol) or 4, one or more arbitrary proportion combinations in 4 '-thiobis (6-tertiary butyl meta-cresol).
Described lubricant is one or more arbitrary proportion combinations in calcium stearate, barium stearate and the Zinic stearas.
A kind of anti-static polycarbonate/polyester alloy material preparation method may further comprise the steps:
1) polycarbonate, polyester and graphitized carbon black is lower dry 12 ~ 24 hours at 100 ~ 110 ℃;
2) with 1 ~ 4% compatilizer, 0.01 ~ 0.05% transesterification catalyst, 0.1 ~ 0.5% oxidation inhibitor, 0 ~ 5% thermo-stabilizer and 0.2 ~ 1% lubricant high-speed mixer and mixing 10 ~ 20 minutes;
3) mixture, 50 ~ 70% polycarbonate and 10 ~ 30% polyester with step 2 gained drop in the Banbury mixer, until melting;
4) 5 ~ 25% graphitized carbon blacks are dropped in the Banbury mixer, the kneading time is 5 ~ 8 minutes, and temperature is 270 ~ 290 ℃;
5) melt that step 4 is obtained is sent in the twin screw extruder, and the rotating speed of forcing machine is 150 ~ 300 rev/mins, melt extrudes granulation under 260 ~ 280 ℃ of temperature.
For the ease of the present invention is further understood, now describe the present invention in conjunction with specific embodiments:
Embodiment 1
The data of giving according to table 1 embodiment 1, at first the Japanese Supreme Being people L-1259Y of company polycarbonate, Japanese Supreme Being people's company's T R 850 polyester 100 ℃ of lower forced air dryings 12 hours; Then with dihydroxyphenyl propane solid epoxy, calcium stearate, triethyl phosphate, the tricresyl phosphite (2 of epoxy equivalent (weight) 699 ~ 700g/eq, the 4-di-tert-butyl-phenyl) ester and 2,2 methylene radical-two (4-methyl-6-tert-butylphenol) according to the composition of mass ratio 2:1, Glacial acetic acid lanthanum high-speed mixer and mixing 15 minutes, mixture in the high mixer is dropped in the Banbury mixer with polycarbonate, polyester, until melting; Cabot VULCANXC72 graphitized carbon black is dropped in the Banbury mixer again and mediated 8 minutes, mediating temperature is 280 ℃; The melt that at last the Banbury mixer kneading is obtained is sent in the twin screw extruder and is melt extruded, granulation, the rotating speed of forcing machine is 150 rev/mins, forcing machine one district's temperature is 260 ~ 265 ℃, two district's temperature are 265 ~ 270 ℃, three district's temperature are 270 ~ 275 ℃, and four district's temperature are 275 ~ 280 ℃, 275 ~ 280 ℃ of head temperatures.Products obtained therefrom is carried out performance test, and its test data sees Table 1.
Embodiment 2
The data of giving according to table 1 embodiment 1, at first the Japanese Supreme Being people L-1259Y of company polycarbonate, Japanese Supreme Being people's company's T R 850 polyester 100 ℃ of lower forced air dryings 12 hours; Then with dihydroxyphenyl propane solid epoxy, calcium stearate, triphenyl phosphite, the tricresyl phosphite (2 of epoxy equivalent (weight) 600 ~ 700g/eq, the 4-di-tert-butyl-phenyl) ester according to the composition of mass ratio 2:1, acetyl ethyl ketone lanthanum high-speed mixer and mixing 15 minutes, mixture in the high mixer is dropped in the Banbury mixer with polycarbonate, polyester, until melting; Cabot VULCANXC72 graphitized carbon black is dropped in the Banbury mixer again and mediated 5 minutes, mediating temperature is 270 ℃; The melt that at last the Banbury mixer kneading is obtained is sent in the twin screw extruder and is melt extruded, granulation, the rotating speed of forcing machine is 200 rev/mins, forcing machine one district's temperature is 250 ~ 255 ℃, two district's temperature are 255 ~ 260 ℃, three district's temperature are 255 ~ 260 ℃, and four district's temperature are 260 ~ 265 ℃, 260 ~ 265 ℃ of head temperatures.Products obtained therefrom is carried out performance test, and its test data sees Table 1.
Embodiment 3
The data of giving according to table 1 embodiment 1, at first the Japanese Supreme Being people L-1259Y of company polycarbonate, Japanese Supreme Being people's company's T R 850 polyester 100 ℃ of lower forced air dryings 12 hours; Then with dihydroxyphenyl propane solid epoxy, barium stearate, the triphenyl phosphite, two (2 of epoxy equivalent (weight) 3000 ~ 3500g/eq, the 4-di-tert-butyl-phenyl) pentaerythritol diphosphites oxidation inhibitor and β-(4-hydroxy phenyl-3, the 5-di-t-butyl) the positive octadecanol ester combination of propionic acid, its mass ratio is that the composition, Glacial acetic acid cerium of 1:1 was high-speed mixer and mixing 20 minutes, mixture in the high mixer is dropped in the Banbury mixer with polycarbonate, polyester, until melting; Cabot VULCANXC72 graphitized carbon black is dropped in the Banbury mixer again and mediated 8 minutes, mediating temperature is 280 ℃; The melt that at last the Banbury mixer kneading is obtained is sent in the twin screw extruder and is melt extruded, granulation, the rotating speed of forcing machine is 250 rev/mins, forcing machine one district's temperature is 255 ~ 260 ℃, two district's temperature are 260 ~ 265 ℃, three district's temperature are 265 ~ 270 ℃, and four district's temperature are 270 ~ 275 ℃, 270 ~ 265 ℃ of head temperatures.Products obtained therefrom is carried out performance test, and its test data sees Table 1.
Embodiment 4
The data of giving according to table 1 embodiment 1, at first the Japanese Supreme Being people L-1259Y of company polycarbonate, Japanese Supreme Being people's company's T R 850 polyester 100 ℃ of lower forced air dryings 12 hours; Then with dihydroxyphenyl propane solid epoxy, Zinic stearas, the triphenylphosphate, 2 of epoxy equivalent (weight) 700 ~ 800g/eq, 2 ' methylene radical-two (4-methyl-6-tert-butylphenol), monobutyl three isocaprylic acid tin were high-speed mixer and mixing 20 minutes, mixture in the high mixer is dropped in the Banbury mixer with polycarbonate, polyester, until melting; Cabot VULCANXC72 graphitized carbon black is dropped in the Banbury mixer again and mediated 8 minutes, mediating temperature is 300 ℃; The melt that at last the Banbury mixer kneading is obtained is sent in the twin screw extruder and is melt extruded, granulation, the rotating speed of forcing machine is 300 rev/mins, forcing machine one district's temperature is 260 ~ 265 ℃, two district's temperature are 265 ~ 270 ℃, three district's temperature are 270 ~ 275 ℃, and four district's temperature are 275 ~ 280 ℃, 280 ~ 275 ℃ of head temperatures.Products obtained therefrom is carried out performance test, and its test data sees Table 1.
Embodiment 5
The data of giving according to table 1 embodiment 1, at first the K2012 terephthalic acid-ethylene glycol of the Japanese Supreme Being people L-1259Y of company polycarbonate, Korea S SK company-Isosorbide-5-Nitrae cyclohexanedimethanol copolyesters (PETG) 100 ℃ of lower forced air dryings 12 hours; Then with dihydroxyphenyl propane solid epoxy, Zinic stearas, the triphenylphosphate, 2 of epoxy equivalent (weight) 1000 ~ 1500g/eq, 2 ' methylene radical-two (4-methyl-6-tert-butylphenol), monobutyl three isocaprylic acid tin were high-speed mixer and mixing 20 minutes, mixture in the high mixer is dropped in the Banbury mixer with polycarbonate, polyester, until melting; Cabot VULCANXC72 graphitized carbon black is dropped in the Banbury mixer again and mediated 8 minutes, mediating temperature is 270 ℃; The melt that at last the Banbury mixer kneading is obtained is sent in the twin screw extruder and is melt extruded, granulation, the rotating speed of forcing machine is 150 rev/mins, forcing machine one district's temperature is 250 ~ 255 ℃, two district's temperature are 255 ~ 260 ℃, three district's temperature are 260 ~ 265 ℃, and four district's temperature are 260 ~ 265 ℃, 265 ~ 270 ℃ of head temperatures.Products obtained therefrom is carried out performance test, and its test data sees Table 1.
Table 1
| Form | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Polycarbonate | 50% | 70% | 56.15% | 56.49% | 51.49% |
| Polyester | 21.69% | 12.19% | 30% | 10% | 15% |
| Graphitized carbon black | 25% | 10% | 5% | 25% | 25% |
| Compatilizer | 2% | 4% | 3% | 2% | 2% |
| Transesterification catalyst | 0.01% | 0.01% | 0.05% | 0.01% | 0.01% |
| Lubricant | 0.8% | 0.5% | 0.3% | 1% | 1% |
| Oxidation inhibitor | 0.5% | 0.3% | 0.5% | 0.5% | 0.5% |
| Thermo-stabilizer | --- | 3% | 5% | 5% | 5% |
| Tensile strength (MPa) ASTM D882 | 52 | 68 | 65 | 57 | 66 |
| Elongation at break (%) ASTM D882 | 8.8 | 11.0 | 9.8 | 7.1 | 10.3 |
| Shock strength (breach, KJ/m 2）ASTM D882 | 4.7 | 5.2 | 5.1 | 4.3 | 5.6 |
| Volume specific resistance (Ω cm) ASTM D257 | 1.00E+5 | 1.00E+6 | 1.00E+10 | 1.00E+5 | 1.00E+5 |
Claims (10)
1. anti-static polycarbonate/polyester alloy material, it is characterized in that: this material comprises following component graphitized carbon black 5 ~ 25%, polycarbonate 50 ~ 70%, polyester 10 ~ 30%, transesterification catalyst 0.01 ~ 0.05%, compatilizer 1 ~ 4%, oxidation inhibitor 0.1 ~ 0.5%, lubricant 0.2 ~ 1% by weight percentage;
Described compatilizer is the dihydroxyphenyl propane solid epoxy, and described polycarbonate is bisphenol-a polycarbonate.
2. anti-static polycarbonate as claimed in claim 1/polyester alloy material is characterized in that: also comprise by weight percentage 0 ~ 5% thermo-stabilizer in this material.
3. anti-static polycarbonate as claimed in claim 1 or 2/polyester alloy material, it is characterized in that: described polyester is ethylene glycol, hexylene glycol, propylene glycol, butyleneglycol, 1, one or more arbitrary proportion combinations in 4-cyclohexanedimethanol, neopentyl glycol and the terephthalyl alcohol and one or more arbitrary proportion combinations in terephthalic acid, m-phthalic acid, cyclohexane cyclohexanedimethanodibasic, pentanedioic acid, hexanodioic acid and the suberic acid, the copolyesters that carries out polymerization.
4. anti-static polycarbonate as claimed in claim 1 or 2/polyester alloy material, the melting index of described polycarbonate are 3 ~ 15 g/10min (300 ℃/1.2kg, ISO1133).
5. anti-static polycarbonate as claimed in claim 1 or 2/polyester alloy material, the DBP absorption value of described graphitized carbon black is that 300 ~ 600ml/100g (ASTM D 2414), resistance are less than 150 Ω cm(Philips-Method), tap density is greater than 120g/l (ASTM D 1513).
6. anti-static polycarbonate as claimed in claim 1 or 2/polyester alloy material, described dihydroxyphenyl propane solid epoxy, its epoxy equivalent (weight) are 800 ~ 3500g/eq (GB/T 4612-2008).
7. anti-static polycarbonate as claimed in claim 1 or 2/polyester alloy material, described transesterification catalyst is a kind of or its combination in Dibutyltin oxide, Mono-n-butyltin, Mono-n-butyltin muriate, monobutyl three isocaprylic acid tin, dibutyl tin acetate, Glacial acetic acid cerium, acetyl ethyl ketone cerium, Glacial acetic acid lanthanum and the acetyl ethyl ketone lanthanum.
8. anti-static polycarbonate as claimed in claim 1 or 2/polyester alloy material, described oxidation inhibitor is tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester, two (2, the 4-di-tert-butyl-phenyl) tetramethylolmethane diphosphorous acid fat, four [3-(3,5-di-t-butyl-4-hydroxyphenyl) propionic acid] quaternary amyl alcohol ester, β-(4-hydroxy phenyl-3, the 5-di-t-butyl) the positive octadecanol ester of propionic acid, 2, the 6-di-tert-butyl-4-methy phenol, 2,2 ' methylene radical-two (4-methyl-6-tert-butylphenol), 4,4 '-thiobis (the 6-tertiary butyl-3-methylphenol) or 4, one or more arbitrary proportion combinations in 4 '-thiobis (6-tertiary butyl meta-cresol).
9. anti-static polycarbonate/polyester alloy material preparation method as claimed in claim 1 is characterized in that, may further comprise the steps:
1) with 1 ~ 4% compatilizer, 0.01 ~ 0.05% transesterification catalyst, 0.1 ~ 0.5% oxidation inhibitor, 0 ~ 5% thermo-stabilizer and 0.2 ~ 1% lubricant high-speed mixer and mixing 10 ~ 20 minutes;
2) mixture, 50 ~ 70% polycarbonate and 10 ~ 30% polyester with step 1 gained drop in the Banbury mixer, until melting;
3) 5 ~ 25% graphitized carbon blacks are dropped in the Banbury mixer, the kneading time is 5 ~ 8 minutes, and temperature is 270 ~ 290 ℃;
4) melt that step 3 is obtained is sent in the twin screw extruder, and the rotating speed of forcing machine is 150 ~ 300 rev/mins, melt extrudes granulation under 260 ~ 280 ℃ of temperature.
10. anti-static polycarbonate as claimed in claim 9/polyester alloy material preparation method is characterized in that: also comprise before the described step 1 polycarbonate, polyester and graphitized carbon black 100 ~ 110 ℃ of steps of lower dry 12 ~ 24 hours.
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